CN114618414B - Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof - Google Patents
Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof Download PDFInfo
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- CN114618414B CN114618414B CN202210426384.8A CN202210426384A CN114618414B CN 114618414 B CN114618414 B CN 114618414B CN 202210426384 A CN202210426384 A CN 202210426384A CN 114618414 B CN114618414 B CN 114618414B
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- 238000000746 purification Methods 0.000 title claims abstract description 88
- NMEZJSDUZQOPFE-UHFFFAOYSA-N Cyclohex-1-enecarboxylic acid Chemical compound OC(=O)C1=CCCCC1 NMEZJSDUZQOPFE-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 81
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims description 36
- 239000012528 membrane Substances 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000110 cooling liquid Substances 0.000 claims description 7
- 238000005260 corrosion Methods 0.000 claims description 7
- 230000007797 corrosion Effects 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- AHHKQEGTXVWSBX-UHFFFAOYSA-N cyclohexene formic acid Chemical compound C(=O)O.C(=O)O.C1=CCCCC1 AHHKQEGTXVWSBX-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims 5
- 238000001914 filtration Methods 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 229940117803 phenethylamine Drugs 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1893—Membrane reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a reaction kettle for purifying cyclohexene carboxylic acid and a purifying method thereof, relates to the technical field of chemical industry, and aims to solve the problem that the working energy consumption of a cyclohexene carboxylic acid purifying device is relatively high because the utilization efficiency of purifying and filtering energy sources in the purifying reaction kettle is low. The upper end of reaction furnace casing is provided with agitator motor, the inside of reaction furnace casing is provided with the (mixing) shaft, the outside of (mixing) shaft is provided with first stirring purification pole support, the below of first stirring purification pole support is provided with the second stirring purification pole support, the lower extreme of reaction furnace casing is provided with the outer support all around, the lower extreme of reaction furnace casing is provided with row's material pipe, the upper end both sides of reaction furnace casing are provided with inlet pipe, heating pipe respectively, one side below of inlet pipe is provided with the water pipe, the inside of reaction furnace casing is provided with the water conservancy diversion dish, the lower extreme of water conservancy diversion dish is provided with porous sieve cover.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a reaction kettle for purifying cyclohexene carboxylic acid and a purification method thereof.
Background
In conventional devices, such as application number: 201911372043.1; the name is: s-3-cyclohexene carboxylic acid and its refining method. The device comprises: mixing, stirring and refluxing the S-3-cyclohexene carboxylic acid crude product, R-a-phenethylamine and ethyl acetate, and filtering to obtain S-3-cyclohexene carboxylic acid-R-a-phenethylamine salt, wherein the S-3-cyclohexene carboxylic acid crude product refers to S-3-cyclohexene carboxylic acid with an ee value less than 97%; mixing the S-3-cyclohexenoic acid-R-a-phenethylamine salt with ethanol, crystallizing, and filtering to obtain a recrystallized material; mixing and stirring dichloromethane, water and the recrystallized material, separating liquid, collecting an organic layer, and carrying out distillation treatment on the organic layer to obtain the S-3-cyclohexene carboxylic acid. The refining method of the S-3-cyclohexene carboxylic acid provided by the invention can enable the ee value of the prepared S-3-cyclohexene carboxylic acid to reach more than 99%, and simultaneously, the resolving agent R-phenethylamine is recycled, so that the cost is saved.
However, the cyclohexene carboxylic acid purification device has low purification and filtration energy utilization efficiency in the purification reaction kettle, so that the problem of higher working energy consumption of the cyclohexene carboxylic acid purification device is caused; therefore, the existing requirements are not met, and a reaction kettle for purifying cyclohexene carboxylic acid and a purification method thereof are provided.
Disclosure of Invention
The invention aims to provide a reaction kettle for purifying cyclohexene carboxylic acid and a purifying method thereof, which are used for solving the problem that the working energy consumption of the cyclohexene carboxylic acid purifying device is higher because the purifying and filtering energy utilization efficiency in the purifying reaction kettle is low in the existing cyclohexene carboxylic acid purifying device provided in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the utility model provides a cyclohexenecarboxylic acid is reation kettle for purification, includes the reacting furnace casing, the upper end of reacting furnace casing is provided with agitator motor, the inside of reacting furnace casing is provided with the (mixing) shaft, and (mixing) shaft and agitator motor transmission are connected, the outside of (mixing) shaft is provided with first stirring purification pole support, and first stirring purification pole support and (mixing) shaft welded connection, the below of first stirring purification pole support is provided with second stirring purification pole support, and second stirring purification pole support and (mixing) shaft welded connection, the lower extreme of reacting furnace casing is provided with the outer support all around, and outer support and reacting furnace casing bolt fixed connection, the lower extreme of reacting furnace casing is provided with row's material pipe, and row material pipe and reacting furnace casing welded connection, the upper end both sides of reacting furnace casing are provided with inlet pipe, heating pipe respectively, one side below of inlet pipe is provided with the water pipe, and water pipe and reacting furnace casing pipe flange connection, the inside of reacting furnace casing is provided with the water conservancy diversion dish, and water conservancy diversion dish and reacting furnace casing's inner wall welded connection, the lower extreme of water conservancy diversion dish and reacting furnace casing is provided with porous sieve cover, and integrative shaping sieve cover.
Preferably, each purifying rod is provided with a connecting shaft inside, and the connecting shafts are respectively connected with the first stirring purifying rod support and the second stirring purifying rod support through rotating shafts, and the outer wall of the purifying rod is provided with a porous shell.
Preferably, a purification plate is arranged on the outer side of the connecting shaft in a circle, the purification plate is connected with the inner wall of the purification rod in a welded mode, a cooling plate is arranged in each purification plate, and corrosion-resistant silica gel grooves are formed in two sides of each cooling plate.
Preferably, each corrosion-resistant silica gel groove's outside all is provided with one-way storage membrane, and one-way storage membrane and cooling plate draw-in groove fixed connection, the both sides of purification board all are provided with porous membrane.
Preferably, the cooling plates are each provided with a cooling liquid inside.
Preferably, a soaking plate is arranged outside the cooling liquid, and the soaking plate is welded and connected with the inner wall of the cooling plate.
Preferably, the lower ends of the first stirring and purifying rod support and the second stirring and purifying rod support are respectively provided with a purifying rod, and the purifying rods are connected with the first stirring and purifying rod support and the second stirring and purifying rod support through rotating shafts.
Preferably, a connecting shaft bearing is arranged at the lower end of the stirring shaft, the connecting shaft bearing is fixedly connected with the porous screen cover through bolts, and the connecting shaft bearing is connected with the stirring shaft bearing.
Preferably, the application method of the reaction kettle for purifying cyclohexene carboxylic acid comprises the following steps of:
step one: the reaction furnace comprises a reaction furnace shell, a stirring motor, a stirring shaft, a first stirring and purifying rod support, a second stirring and purifying rod support, a heating pipe, a flow guide disc, a porous screen cover and a connecting shaft, wherein materials are firstly input from a feed pipe, then a water adding pipe controls the input of water quantity, the stirring motor controls the stirring shaft to rotate, the mixture is fully stirred, the materials are fully stirred by the purifying rods at the lower ends of the first stirring and purifying rod support and the second stirring and purifying rod support, the materials are heated by the heating pipe, and the precipitation of cyclohexene formic acid is accelerated;
step two: when the cyclohexene carboxylic acid is heated and stirred, the cyclohexene carboxylic acid can pass through the porous shell of the purification rod and then is deposited on two sides of the interior of the purification plate, the surface area contacted with the cyclohexene carboxylic acid is greatly increased by the purification plate, the cyclohexene carboxylic acid can be accelerated to be adhered to the purification plate to finish purification, the cyclohexene carboxylic acid passes through the porous permeable membrane and is deposited on the unidirectional storage membrane, after the deposition is finished, the unidirectional storage membrane can be detached from the groove of the cooling plate, the unidirectional storage membrane can prevent the cyclohexene carboxylic acid from overflowing, and the purification efficiency of the cyclohexene carboxylic acid is greatly improved;
step three: the cooling liquid inside the cooling plate can quickly absorb the heat of the cooling plate, so that the temperature difference between the two sides of the cooling plate and the external environment is formed, the cyclohexene carboxylic acid flows towards the inside of the unidirectional storage film, the fixation of the cyclohexene carboxylic acid inside the unidirectional storage film is greatly improved, the accelerated purification and separation of the cyclohexene carboxylic acid is realized, and the problem that the working energy consumption of the cyclohexene carboxylic acid purification device is higher due to the fact that the utilization efficiency of purification and filtration energy sources inside a purification reaction kettle is low in the existing cyclohexene carboxylic acid purification device is solved.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the arrangement of the reaction furnace shell, the stirring motor, the stirring shaft, the first stirring and purifying rod support, the second stirring and purifying rod support, the heating pipe, the guide disc, the porous screen cover and the connecting shaft, materials are firstly input from the feeding pipe, then the water adding pipe controls the input of water quantity, the stirring motor controls the stirring shaft to rotate, the mixture is fully stirred, the materials are fully stirred by the purifying rods at the lower ends of the first stirring and purifying rod support and the second stirring and purifying rod support, the heating pipe heats the materials, and the precipitation of cyclohexene formic acid is accelerated.
2. Through the setting of purification board, when cyclohexene carboxylic acid is heated and stirred, the porous shell of purification pole can be passed to cyclohexene carboxylic acid, later deposit in the inside both sides of purification board, the purification board has greatly improved the surface area with cyclohexene carboxylic acid contact for cyclohexene carboxylic acid can accelerate to adhere to and accomplish the purification at the purification board, the cyclohexene carboxylic acid passes porous osmotic membrane and deposits on one-way storage membrane, after the deposit, can dismantle one-way storage membrane from the recess of cooling plate, one-way storage membrane can prevent cyclohexene carboxylic acid excessive, greatly improved the purification efficiency to cyclohexene carboxylic acid.
3. Through the setting of cooling plate, the inside coolant liquid of cooling plate can absorb the heat of cooling plate fast for the cooling plate both sides form with external environment between the temperature difference, accelerate cyclohexene carboxylic acid and accomodate the membrane in one direction and flow to its inside, greatly improved cyclohexene carboxylic acid at the inside fixed of membrane is accomodate to one direction, thereby realized the purification separation with higher speed to cyclohexene carboxylic acid, solved current cyclohexene carboxylic acid purification device, because purification reation kettle is inside to purify the energy utilization efficiency not high, cause cyclohexene carboxylic acid purification device work energy consumption higher problem.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic cross-sectional view of a purifying rod according to the present invention;
FIG. 3 is a schematic view showing the internal structure of the purification plate of the present invention;
FIG. 4 is a schematic view showing the internal structure of the cooling plate according to the present invention;
FIG. 5 is an enlarged view of a portion of the invention at A;
in the figure: 1. a reaction furnace housing; 2. a stirring motor; 3. a stirring shaft; 4. a first stirring and purifying rod bracket; 5. a second stirring and purifying rod bracket; 6. a purifying rod; 7. a feed pipe; 8. heating pipes; 9. a water supply pipe; 10. an outer bracket; 11. a discharge pipe; 12. a deflector disc; 13. a porous screen cover; 14. a connecting shaft; 15. a purification plate; 16. a porous housing; 17. a porous permeable membrane; 18. a cooling plate; 19. a corrosion-resistant silica gel groove; 20. a one-way storage film; 21. a cooling liquid; 22. a soaking plate; 23. and a connecting shaft bearing.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1-5, an embodiment of the present invention is provided: the utility model provides a reaction kettle for cyclohexene carboxylic acid purification, including reaction furnace casing 1, reaction furnace casing 1's upper end is provided with agitator motor 2, reaction furnace casing 1's inside is provided with (mixing) shaft 3, and (mixing) shaft 3 and (mixing) motor 2 transmission are connected, agitator shaft 3's outside is provided with first stirring purification pole support 4, and first stirring purification pole support 4 and (mixing) shaft 3 welded connection, first stirring purification pole support 4's below is provided with second stirring purification pole support 5, and second stirring purification pole support 5 and (mixing) shaft 3 welded connection, reaction furnace casing 1's lower extreme is provided with outer support 10 all around, and outer support 10 and reaction furnace casing 1 bolted connection, reaction furnace casing 1's lower extreme is provided with row material pipe 11, and row material pipe 11 and reaction furnace casing 1 welded connection, reaction furnace casing 1's upper end both sides are provided with inlet pipe 7 respectively, heating pipe 8, one side below of inlet pipe 7 is provided with water pipe 9 and reaction furnace casing 1 pipe flange connection, reaction furnace casing 1's inside is provided with water conservancy diversion dish 12, and water conservancy diversion dish 12 and reaction furnace casing 1's inner wall 12 are connected with (mixing) shaft 3 welded connection, and the porous sieve 13 sets up the integrative sieve of porous sieve 13 with the lower extreme of reaction furnace casing 1, and sieve 13 welded connection.
Further, a connecting shaft 14 is arranged in each purifying rod 6, the connecting shafts 14 are respectively connected with the first stirring purifying rod support 4 and the second stirring purifying rod support 5 in a rotating shaft mode, and a porous shell 16 is arranged on the outer wall of each purifying rod 6.
Further, a purification plate 15 is arranged on the outer circumference of the connecting shaft 14, the purification plate 15 is welded with the inner wall of the purification rod 6, a cooling plate 18 is arranged in each purification plate 15, and corrosion-resistant silica gel grooves 19 are formed in two sides of each cooling plate 18.
Further, the outside of each corrosion-resistant silica gel groove 19 is provided with a unidirectional storage film 20, and the unidirectional storage film 20 is fixedly connected with the clamping groove of the cooling plate 18, and the two sides of the purification plate 15 are provided with porous membranes 17.
Further, the inside of each cooling plate 18 is provided with a cooling liquid 21.
Further, a soaking plate 22 is provided outside the coolant 21, and the soaking plate 22 is welded to the coolant 21.
Further, the lower ends of the first stirring and purifying rod support 4 and the second stirring and purifying rod support 5 are respectively provided with a purifying rod 6, and the purifying rods 6 are connected with the first stirring and purifying rod support 4 and the second stirring and purifying rod support 5 in a rotating shaft manner.
Further, a connecting shaft bearing 23 is arranged at the lower end of the stirring shaft 3, the connecting shaft bearing 23 is fixedly connected with the porous screen cover 13 through bolts, and the connecting shaft bearing 23 is connected with the stirring shaft 3 through a bearing.
Further, the application method of the reaction kettle for purifying the cyclohexene carboxylic acid comprises the following steps:
step one: the reaction furnace comprises a reaction furnace shell 1, a stirring motor 2, a stirring shaft 3, a first stirring and purifying rod support 4, a second stirring and purifying rod support 5, a heating pipe 8, a guide disc 12, a porous screen cover 13 and a connecting shaft 14, wherein materials are firstly input from a feed pipe 7, then a water adding pipe 9 controls the input of water quantity, the stirring motor 2 controls the stirring shaft 3 to rotate, the mixture is fully stirred, a purifying rod 6 at the lower end of the first stirring and purifying rod support 4 and the lower end of the second stirring and purifying rod support 5 fully stirs the materials, and the heating pipe 8 heats the materials to accelerate precipitation of cyclohexene formic acid;
step two: when the cyclohexene carboxylic acid is heated and stirred, the cyclohexene carboxylic acid passes through the porous shell 16 of the purification rod 6 and then is deposited on two sides of the inside of the purification plate 15, the surface area of the purification plate 15 contacted with the cyclohexene carboxylic acid is greatly increased, the cyclohexene carboxylic acid can be quickly attached to the purification plate 15 to finish purification, the cyclohexene carboxylic acid passes through the porous permeable membrane 17 and is deposited on the unidirectional containing membrane 20, after the deposition is finished, the unidirectional containing membrane 20 can be detached from the groove of the cooling plate 18, the unidirectional containing membrane 20 can prevent the cyclohexene carboxylic acid from overflowing, and the purification efficiency of the cyclohexene carboxylic acid is greatly improved;
step three: the cooling liquid 21 inside the cooling plate 18 can quickly absorb the heat of the cooling plate 18, so that the temperature difference between the two sides of the cooling plate 18 and the external environment is formed, the cyclohexene carboxylic acid is accelerated to flow into the unidirectional storage film 20, the fixation of the cyclohexene carboxylic acid inside the unidirectional storage film 20 is greatly improved, the accelerated purification and separation of the cyclohexene carboxylic acid are realized, and the problem that the working energy consumption of the cyclohexene carboxylic acid purification device is relatively high due to the fact that the utilization efficiency of purification and filtration energy sources inside a purification reaction kettle is low in the existing cyclohexene carboxylic acid purification device is solved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (3)
1. The utility model provides a cyclohexenecarboxylic acid purification is with reation kettle, includes reaction furnace casing (1), its characterized in that: the upper end of reaction furnace casing (1) is provided with (mixing) motor (2), the inside of reaction furnace casing (1) is provided with (mixing) shaft (3), and (mixing) shaft (3) and (mixing) motor (2) transmission connection, the outside of (mixing) shaft (3) is provided with first stirring purification pole support (4), and first stirring purification pole support (4) and (mixing) shaft (3) welding, the below of first stirring purification pole support (4) is provided with second stirring purification pole support (5), and second stirring purification pole support (5) and (mixing) shaft (3) welding, the lower extreme of reaction furnace casing (1) is provided with outer support (10) all around, and outer support (10) and reaction furnace casing (1) bolt fixed connection, the lower extreme of reaction furnace casing (1) is provided with row material pipe (11), and row material pipe (11) and reaction furnace casing (1) welding, the upper end both sides of reaction furnace casing (1) are provided with inlet pipe (7), heating pipe (8) respectively, one side below (7) is provided with second stirring purification pole support (5), and adds water pipe (9) and reaction furnace casing (1) and water conservancy diversion dish (12) and reaction furnace casing (1) welding, water pipe (12) and reaction furnace casing (1) inner wall (12), the lower extreme of water conservancy diversion dish (12) is provided with porous sieve cover (13), and porous sieve cover (13) and water conservancy diversion dish (12) integrated into one piece set up, the lower extreme of first stirring purification pole support (4) and second stirring purification pole support (5) all is provided with purification pole (6), the inside of every purification pole (6) all is provided with connecting axle (14), and connecting axle (14) are connected with first stirring purification pole support (4), second stirring purification pole support (5) respectively, purification pole (6) outer wall is provided with porous shell (16), the outside week of connecting axle (14) is provided with purification board (15), and purification board (15) and the inner wall welding of purification pole (6), every the inside of purification board (15) all is provided with cooling plate (18), the both sides of cooling plate (18) all are provided with corrosion-resistant silica gel groove (19), every the outside of corrosion-resistant silica gel groove (19) all is provided with one-way storage membrane (20), and one-way storage membrane (20) and cooling plate (18) are connected with cooling plate (21), every cooling plate (21) are provided with cooling plate (21), every cooling plate (21) are all provided with cooling plate (21).
2. The reaction kettle for purifying cyclohexene carboxylic acid according to claim 1, wherein: the lower end of the stirring shaft (3) is provided with a connecting shaft bearing (23), the connecting shaft bearing (23) is fixedly connected with the porous screen cover (13) through bolts, and the connecting shaft bearing (23) is connected with the stirring shaft (3) through bearings.
3. The method for using a reaction kettle for purifying cyclohexene carboxylic acid as claimed in claim 2, comprising the following steps:
step one: the reaction furnace comprises a reaction furnace shell (1), a stirring motor (2), a stirring shaft (3), a first stirring and purifying rod support (4), a second stirring and purifying rod support (5), a heating pipe (8), a guide disc (12), a porous screen cover (13) and a connecting shaft (14), wherein materials are firstly input from a feeding pipe (7), then the water adding pipe (9) controls the input of water quantity, the stirring motor (2) controls the stirring shaft (3) to rotate, the mixture is fully stirred, a purifying rod (6) at the lower end of the first stirring and purifying rod support (4) and the lower end of the second stirring and purifying rod support (5) fully stirs the materials, the heating pipe (8) heats the materials, and precipitation of cyclohexene formic acid is accelerated;
step two: when the cyclohexene carboxylic acid is heated and stirred, the cyclohexene carboxylic acid passes through the porous shell (16) of the purifying rod (6) and then is deposited on two sides of the inside of the purifying plate (15), the surface area of the purifying plate (15) contacted with the cyclohexene carboxylic acid is increased, the cyclohexene carboxylic acid can be accelerated to adhere to the purifying plate (15) to finish purification, the cyclohexene carboxylic acid passes through the porous permeable membrane (17) and is deposited on the unidirectional containing membrane (20), after the deposition is finished, the unidirectional containing membrane (20) can be detached from the groove of the cooling plate (18), the unidirectional containing membrane (20) can prevent the cyclohexene carboxylic acid from overflowing, and the purifying efficiency of the cyclohexene carboxylic acid is improved;
step three: the cooling liquid (21) in the cooling plate (18) can quickly absorb the heat of the cooling plate (18) so that the temperature difference between the two sides of the cooling plate (18) and the external environment is formed, the accelerated cyclohexene carboxylic acid flows into the unidirectional storage film (20), the fixation of the cyclohexene carboxylic acid in the unidirectional storage film (20) is improved, and the accelerated purification and separation of the cyclohexene carboxylic acid are realized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210426384.8A CN114618414B (en) | 2022-04-22 | 2022-04-22 | Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210426384.8A CN114618414B (en) | 2022-04-22 | 2022-04-22 | Reaction kettle for purifying cyclohexenecarboxylic acid and purification method thereof |
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| Publication Number | Publication Date |
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| CN114618414A CN114618414A (en) | 2022-06-14 |
| CN114618414B true CN114618414B (en) | 2023-11-07 |
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| CN211246531U (en) * | 2019-09-04 | 2020-08-14 | 辽宁东大光明化工科技有限责任公司 | Reation kettle is used in chemical industry purification |
| CN212327615U (en) * | 2019-12-26 | 2021-01-12 | 北京瑞芬生物科技股份有限公司 | Modular low-pressure ursodesoxycholic acid filtering device |
| CN212882411U (en) * | 2020-06-12 | 2021-04-06 | 黄发旺 | Chemical industry reation kettle with filtering capability just is convenient for material recovery |
| WO2021174809A1 (en) * | 2020-03-06 | 2021-09-10 | 深圳第三代半导体研究院 | Method and device for purifying multi-dimensional nanomaterial |
| CN113967441A (en) * | 2021-11-17 | 2022-01-25 | 连云港瑞邦药业有限公司 | Purification and filling device and method for calcium gluconate production |
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| DE102004044638A1 (en) * | 2004-09-13 | 2006-03-30 | Stockhausen Gmbh | Purification of a (meth) acrylic acid contained distillation bottoms product by crystallization |
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| CN210595859U (en) * | 2019-09-26 | 2020-05-22 | 山东省越兴化工有限公司 | A purification device for m-toluic acid production |
| CN110960879A (en) * | 2019-12-17 | 2020-04-07 | 郑州超之肽生物技术有限公司 | Purification device for volatile chemical organic compounds |
| CN212327615U (en) * | 2019-12-26 | 2021-01-12 | 北京瑞芬生物科技股份有限公司 | Modular low-pressure ursodesoxycholic acid filtering device |
| WO2021174809A1 (en) * | 2020-03-06 | 2021-09-10 | 深圳第三代半导体研究院 | Method and device for purifying multi-dimensional nanomaterial |
| CN212882411U (en) * | 2020-06-12 | 2021-04-06 | 黄发旺 | Chemical industry reation kettle with filtering capability just is convenient for material recovery |
| CN113967441A (en) * | 2021-11-17 | 2022-01-25 | 连云港瑞邦药业有限公司 | Purification and filling device and method for calcium gluconate production |
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| CN114618414A (en) | 2022-06-14 |
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